US4037331A - Freeze-drying apparatus - Google Patents

Freeze-drying apparatus Download PDF

Info

Publication number
US4037331A
US4037331A US05/650,000 US65000076A US4037331A US 4037331 A US4037331 A US 4037331A US 65000076 A US65000076 A US 65000076A US 4037331 A US4037331 A US 4037331A
Authority
US
United States
Prior art keywords
enclosure
particles
vanes
opening
frusto
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
US05/650,000
Other languages
English (en)
Inventor
Jacques Brilloit
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Original Assignee
LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude filed Critical LAir Liquide SA pour lEtude et lExploitation des Procedes Georges Claude
Application granted granted Critical
Publication of US4037331A publication Critical patent/US4037331A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Images

Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B5/00—Drying solid materials or objects by processes not involving the application of heat
    • F26B5/04—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum
    • F26B5/06—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum the process involving freezing

Definitions

  • the present invention relates to apparatus for freeze-drying particles of material, of the kind which has a rotary sublimating enclosure equipped with agitator or tumbler vanes which normally operate about a horizontal axis.
  • Freeze-drying apparatus having a sublimating enclosure fitted with a frusto-conical set of vanes, the vanes each being adapted to form catchment troughs when they passed through a lower zone of the said enclosure and to form chutes emptying into an axial discharge area when they ascended.
  • a downwardly inclined discharge passage which began at the said axial zone, preferably by placing a discharge deflector in the path of the particles as they flowed from the said vanes towards the axial area.
  • An apparatus of this type has undeniable advantages, due to the fact that it is possible to discharge the particles automatically at the end of the freeze-drying process, which, if required, allows them to be kept under vacuum or in a controlled atmosphere. A completely cylindrical freeze-drying enclosure will not allow discharge by this method.
  • agitating the particles during sublimation by means of a frusto-conical set of vanes of the kind described above has the drawback that the agitation is too violent, being far more vigorous than that from a cylindrical set of vanes, and results in the formation of "fines", which are particularly undesirable in certain applications.
  • the invention provides a freeze-drying apparatus is characterised in that it has, besides at least one catchment and discharge vane, a cylindrical set of vanes which continue on from the said catchment and discharge vane, and means for transferring the particles from the said cylindrical set of vanes to the said catchment and discharge vane.
  • These transfer means are advantageously formed by deflectors which are so arranged between the vanes making up the cylindrical set as to form a helical transfer screw.
  • FIG. 1 is a schematic axial section through a freeze-drying apparatus according to the invention
  • FIG. 2 is a schematic cross-section on line II--II of FIG. 1 of the sublimating cylinder of the freeze-drying apparatus
  • FIG. 3 is an axial section similar to FIG. 1 showing in particular the means of driving the sublimating cylinder
  • FIG. 4 is a partly cut-away perspective view of said cylinder
  • FIGS. 5 and 6 are developed views, in plan and perspective respectively, of the inside wall of said cylinder and
  • FIG. 7 is a schematic axial section through a modified embodiment according to the invention.
  • a freeze-drying apparatus has a sublimating enclosure or cylinder 1 which is mounted to rotate about a horizontal axis in bearings 2 and 3, being driven by a motor 4 via a chain 5 which engages with a large diameter axial conduit 6 which is attached to the mouth of an appropriate opening 7 in cylinder 1.
  • the axial conduit 6 is connected (FIG. 1), by a frusto-conical passage 8, to a cyclone separator 9 which has a condenser 10 using liquid nitrogen.
  • the liquid nitrogen is introduced at 11 and removed at 12.
  • a wide filter 13 is positioned inside the cylinder to block opening 7.
  • the sublimating cylinder 1 is located in a fixed, coaxial, cylindrical housing, whose end-walls 16 and 17 form supports for bearings 2 and 3 and of which the lower part forms a tank 18 for a heating liquid.
  • the temperature of this liquid is closely maintained by means of two feed tanks 20 and 21, one of which may exercise a cooling function for example, by means of liquid nitrogen which is injected into circuit 22 in tank 20, and the other of which may exercise a heating function by means of steam which is injected into circuit 23 in tank 21 and by means of an auxiliary resistance heater 24.
  • a coolant supply tank 25 Also provided is a coolant supply tank 25.
  • the cylinder 1 is mainly formed by a cylindrical portion 28 which terminates in two frusto-conical end portions 29 and 30, which represent respectively the end at which the particles are introduced and discharged and the end at which the sublimation vapours are extracted.
  • frusto-conical part 29 On the other hand, which is situated at the end where the passage for introducing and removing the particles is situated, performs a function to which reference will soon be made.
  • frusto-conical part 29 At its end of smaller cross-section, frusto-conical part 29 has an opening 31 which communicates, via a sealed bearing 32, on the one hand with a passage 33 for admitting particles which is downwardly inclined towards 31, and on the other hand with a passage 34 for discharging particles which is downwardly inclined away from opening 31.
  • Admission passage 33 is provided with valves 35, 36 and 37 which allow an inlet lock 38 to be formed for particles which are stored in a storage freezer 39.
  • Discharge passage 34 which is fitted with a valve 40, opens onto a receptacle 41 for freeze-dried particles.
  • the frusto-conical part 29 is provided with a set of vanes 44 which form troughs for catching particles when in their low position and chutes for discharging into opening 31 when they rise. It will be appreciated that the particles are discharged simply as a result of the rotation of the vanes 44 which agitate the particles, assuming that a discharge deflector 45, which is normally in the inoperative position (shown in solid lines in FIG. 1), is rotated through 180° about the axis of the cylinder and is brought to a position 45' (shown as a broken line) in which it catches the particles leaving vanes 44 and thus directs them into discharge passage 34.
  • a discharge deflector 45 which is normally in the inoperative position (shown in solid lines in FIG. 1), is rotated through 180° about the axis of the cylinder and is brought to a position 45' (shown as a broken line) in which it catches the particles leaving vanes 44 and thus directs them into discharge passage 34.
  • the cylindrical part 28 of the cylinder 1 is provided with set of vanes 48 parallel to its axis, the cross-section of which vanes is triangular. Between vanes 48 are positioned discharge guides 49 which are made up of deflecting walls 50 and coaxial blanking-off walls 51 and radial blanking-off walls 52. Guides 49 are positioned in a helical line 53 (FIG. 4) and it can be seen that, when the cylinder 1 turns in direction of rotation f1, the particles which it agitates will move axially in direction F whereas, when cylinder 1 turns in the opposite direction f2, the guides 49, due to their radial walls 52, will have no effect on the particles. In the arrangement described, the frusto-conical wall 29 with the vanes 44 lies in direction F with respect to the cylindrical portion 28 of cylinder 1.
  • the freeze-drying apparatus thus operates as follows: the particles enter through inlet passage 33 and are received, simply by flowing under gravity and by virtue of the action of deflector 45, which is in the raised position, by the vanes 48 in the cylindrical part 28 of cylinder 1, which latter is revolving in direction f2.
  • cylinder 1 continues to rotate in direction f2 and the particles are agitated solely by the vanes 48 in the cylindrical portion 28.
  • the direction of rotation of cylinder 1 is changed from f2 to f1, at the same time as deflector 45 is moved to the lowered position 45'.
  • the particles are then transferred progressively from the vanes 48 in the cylindrical portion 28 to the vanes 44 in the frusto-conical portion 29 and thence, as indicated above, to the discharge passage.
  • vanes 44 and 48 are welded to frusto-conical and cylindrical portions 29 and 28 respectively.
  • a cylindrical sheet may advantageously be folded in such a way as to form both the cylindrical portion 28 and the vanes 48 (FIG. 2). In this way heat is properly transmitted to the particles under all circumstances.
  • a freeze-drying apparatus may be formed with two cylindro-conical enclosures 70 and 71 as described above, in order to be able to subject the particles to different types of treatment.
  • the first sublimating enclosure 70 is equipped with a loading device 73 and a discharge device 74 while the two cylinders are connected axially in line by a valve 75.
  • the second cylinder 71 has a passage 76 which acts as an extraction duct for vapours from both enclosures, and a discharge passage 77.
  • Both cylinders 70 and 71 have portions 78 and 78' with cylindrical sets of vanes and portions 79 and 79' respectively upstream and downstream with frusto-conical sets of vanes, while enclosure 70 alone has a second downstream frusto-conical set of vanes 80, the upstream frusto-conical set 80' in enclosure 71 being optional.
  • the invention is applicable to freeze-drying biological, pharmaceutical and food products.
US05/650,000 1975-01-22 1976-01-19 Freeze-drying apparatus Expired - Lifetime US4037331A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR7501880A FR2298777A2 (fr) 1975-01-22 1975-01-22 Appareil de lyophilisation
FR75.01880 1975-01-22

Publications (1)

Publication Number Publication Date
US4037331A true US4037331A (en) 1977-07-26

Family

ID=9150130

Family Applications (1)

Application Number Title Priority Date Filing Date
US05/650,000 Expired - Lifetime US4037331A (en) 1975-01-22 1976-01-19 Freeze-drying apparatus

Country Status (8)

Country Link
US (1) US4037331A (cs)
JP (1) JPS51126557A (cs)
CH (1) CH584392A5 (cs)
DE (1) DE2601941A1 (cs)
DK (1) DK22076A (cs)
ES (1) ES444426A2 (cs)
FR (1) FR2298777A2 (cs)
GB (1) GB1519735A (cs)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4674198A (en) * 1986-03-17 1987-06-23 Huettlin Herbert Apparatus for granulating, pelleting, and coating and/or drying fluid materials
EP0362888A1 (en) * 1988-10-07 1990-04-11 Freund Industrial Co., Ltd. Appareil d envobage d une poudre ou de granules
EP1139048A1 (en) * 1999-10-07 2001-10-04 Wong, Jo Yuk Rotary dryer
US20040009230A1 (en) * 2000-09-21 2004-01-15 Joel Richard Method for isolating and drying microparticles (microspheres or microcapsules) initially dispersed or suspensed in liquid phase
CN105611838A (zh) * 2013-07-19 2016-05-25 普罗赛索斯耐趣尔斯威尔库有限公司 用于使用微波能量来加速冷冻干燥产品的方法
US11175093B1 (en) * 2020-05-18 2021-11-16 MII Ltd. Vacuum freeze-drying apparatus and vacuum freeze-drying method
US20230100406A1 (en) * 2020-05-18 2023-03-30 Mii, Ltd. Vacuum freeze-drying apparatus and vacuum freeze-drying method
US20240085107A1 (en) * 2021-08-03 2024-03-14 MII Ltd. Freeze-dried product

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4389794A (en) * 1980-12-23 1983-06-28 Bitterly Jack G Vacuum chamber and method of creating a vacuum
FR3133228B1 (fr) * 2022-03-01 2024-04-12 Lyophitech Dispositif de lyophilisation

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2029126A (en) * 1934-03-01 1936-01-28 T L Smith Co Mixing apparatus
US3088222A (en) * 1959-07-01 1963-05-07 Robert C Mace Freeze drying system
US3751820A (en) * 1970-12-16 1973-08-14 Air Liquide Charging and discharging of lyophilisation apparatus

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2029126A (en) * 1934-03-01 1936-01-28 T L Smith Co Mixing apparatus
US3088222A (en) * 1959-07-01 1963-05-07 Robert C Mace Freeze drying system
US3751820A (en) * 1970-12-16 1973-08-14 Air Liquide Charging and discharging of lyophilisation apparatus

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4674198A (en) * 1986-03-17 1987-06-23 Huettlin Herbert Apparatus for granulating, pelleting, and coating and/or drying fluid materials
EP0362888A1 (en) * 1988-10-07 1990-04-11 Freund Industrial Co., Ltd. Appareil d envobage d une poudre ou de granules
EP1139048A1 (en) * 1999-10-07 2001-10-04 Wong, Jo Yuk Rotary dryer
EP1139048A4 (en) * 1999-10-07 2002-10-24 Wong Jo Yuk ROTATING DRYER
US20040009230A1 (en) * 2000-09-21 2004-01-15 Joel Richard Method for isolating and drying microparticles (microspheres or microcapsules) initially dispersed or suspensed in liquid phase
US7354514B2 (en) 2000-09-21 2008-04-08 Ethypharm S.A. Method for isolating and drying microparticles (microspheres or microcapsules) initially dispersed or suspensed in liquid phase
CN105611838A (zh) * 2013-07-19 2016-05-25 普罗赛索斯耐趣尔斯威尔库有限公司 用于使用微波能量来加速冷冻干燥产品的方法
US20160157501A1 (en) * 2013-07-19 2016-06-09 Procesos Naturales Vilkun S.A. Method for accelerating freeze drying produce using microwave energy
US11175093B1 (en) * 2020-05-18 2021-11-16 MII Ltd. Vacuum freeze-drying apparatus and vacuum freeze-drying method
US20230100406A1 (en) * 2020-05-18 2023-03-30 Mii, Ltd. Vacuum freeze-drying apparatus and vacuum freeze-drying method
US11644236B2 (en) * 2020-05-18 2023-05-09 Mii, Ltd. Vacuum freeze-drying apparatus and vacuum freeze-drying method
US20240085107A1 (en) * 2021-08-03 2024-03-14 MII Ltd. Freeze-dried product
US11940214B1 (en) * 2021-08-03 2024-03-26 Mii, Ltd. Freeze-dried product

Also Published As

Publication number Publication date
ES444426A2 (es) 1977-05-16
FR2298777B2 (cs) 1977-07-15
DE2601941A1 (de) 1976-07-29
CH584392A5 (cs) 1977-01-31
GB1519735A (en) 1978-08-02
DK22076A (da) 1976-07-23
FR2298777A2 (fr) 1976-08-20
JPS51126557A (en) 1976-11-04

Similar Documents

Publication Publication Date Title
US4037331A (en) Freeze-drying apparatus
DE3803109C2 (de) Verfahren zum Trocknen von feuchtem Material
DE3844700A1 (de) Verfahren und vorrichtung zur biologischen aufbereitung organischer stoffe
CA1157421A (en) Process and apparatus for desolventizing and drying solvent wet materials
EP2859291A2 (de) Verfahren und maschine zum trocknen von stoffen
US3296709A (en) Rotary drier
KR101899758B1 (ko) 분말 건조장치
US2878581A (en) Dryers
US4369585A (en) Wet and dry roasting apparatus and process for nut, bean and seed-like product
US550035A (en) Extracting and drying apparatus
US4854941A (en) Method and apparatus for drying fine coal
JP4261658B2 (ja) 攪拌処理装置
US3617030A (en) Mixing equipment for dry vegetables
US4401019A (en) Apparatus for thermochemical treatment of crushed straw and or dry fodder mixtures
EP0006751A1 (en) Deflashing apparatus
US3460269A (en) Process and apparatus for vacuum-drying bulk materials
US2811539A (en) Solvent extraction and removal system
US3864841A (en) Rotary dehydrator-granulator
EP1236015B1 (en) Batch sludge dehydrator
CS268151B2 (en) Treatment of moulding sand especially by cooling and mixing and device for making thereof
JPH08136129A (ja) 含水物乾燥処理装置
CN109609262B (zh) 一种湿粕蒸脱机
US4260368A (en) Process and a device for treatment of biologic fuels
US3359649A (en) Apparatus for the heating of bulk material and recovery of vaporizable product therefrom
US2026922A (en) Drier